CN1178861C - Method for preparing gallium nitrate - Google Patents
Method for preparing gallium nitrate Download PDFInfo
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- CN1178861C CN1178861C CNB021241430A CN02124143A CN1178861C CN 1178861 C CN1178861 C CN 1178861C CN B021241430 A CNB021241430 A CN B021241430A CN 02124143 A CN02124143 A CN 02124143A CN 1178861 C CN1178861 C CN 1178861C
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- solution
- gallium
- gallium nitrate
- water
- nitric acid
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Abstract
The present invention relates to a gallium nitrate preparation method which belongs to the technical field of the preparation of gallium nitrate. The preparation method is characterized in that the preparation method comprises the following steps that gallium sesquioxide is dissolved into a nitric acid solution, and the molar ratio of gallium sesquioxide to nitric acid is controlled between 1:18 to 1:6; water adding, heating and vaporizing are carried out repeatedly for 6 to 15 hours until a transparent solution without an irritating smell is formed; the formed solution is heated in a water bath for 8 to 16 hours under the conditions of the water temperature of 40 to 80 DEG C and the systematic pressure of 0.05*10<5> to 0.5*10<5> Pa so as to remove most of the water and the nitric acid; the concentrated solution is placed in nitrogen or air at the temperature of 40 to 80 DEG C so as to be dried for 18 to 36 hours at the normal pressure; consequently, gallium nitrate is obtained. When the obtained gallium nitrate is used for preparing a catalyst used for the control of the lean combustion of nitrogen oxides, the performance of the obtained gallium nitrate is equal to the performance of imported gallium nitrate while the preparation cost of the obtained gallium nitrate is less than one percent of the cost of the imported gallium nitrate.
Description
Technical field
The preparation method of gallium nitrate belongs to the gallium nitrate preparing technical field.
Background technology
Be that the gallium zeolites catalyzer (as Ga-ZSM-5 etc.) of feedstock production and alumina supporter class catalyzer are (as Ga with the gallium nitrate
2O
3-Al
2O
3And SnO
2-Ga
2O
3-Al
2O
3Deng) NOx that produces under the hydrocarbon polymer SCR lean burn condition is had good activity, but with other salt such as the Ga of gallium
2(SO
4)
3And GaCl
3Deng being this two classes catalyzer of feedstock production, its activity is subjected to serious inhibition.In addition, gallium nitrate is used to prepare other catalyzer and also demonstrates purposes widely, Ga
2O
3-Al
2O
3-SiO
2Catalyzer has efficiently as the cracking of hydrocarbon ils; Contain 0.001% gallium in two fat and just can carry out catalysis its polymerization; The catalyzer that contains gallium, iridium and platinum effectively catalysis heptane changes into fragrant substance.
At present foreign literature all obtains with gallium or gallium hydroxide and concentrated nitric acid prepared in reaction about gallium nitrate preparation method's report, the gallium nitrate of its preparation contains the crystal water of some amount, and technology, experiment condition and the relevant parameter of its preparation maintained secrecy (as Sheka at " The Chemistry of Gallium ", P135, report Ga (NO
3)
38H
2The granular crystalline of O prepares), thereby operability is very poor.At present, do not have home-made gallium nitrate product on the domestic market, then cost an arm and a leg, about 160 yuan of the every gram of retail price of gallium nitrate on the domestic market (chemical pure) from U.S.'s import.Therefore, the DOMESTICATION PROBLEM of solution gallium nitrate product has become the task of top priority.
Goal of the invention
The object of the present invention is to provide the gallium nitrate preparation method that a kind of raw material is inexpensive, technology is simple and operability is good.
The invention is characterized in that it contains successively has the following steps:
(1) Gallium trioxide is dissolved in salpeter solution, the mol ratio of control Gallium trioxide and nitric acid is 1: 6-18, during, adding water-heating-evaporation-concentrate-add water again, this operation is 6-15 hour repeatedly, until the transparent solution that has no irritating odor of formation;
(2) at water temperature 40-80 ℃, system pressure 0.05 * 10
5-0.5 * 10
5Under the Pa condition, the solution that step (1) is made was positioned under the condition of water bath heating underpressure distillation 8-16 hour, removed most of water and remaining nitric acid in the middle of the solution, obtained thick concentrated solution;
(3) the thick concentrated solution that step (2) is obtained is placed on temperature 40-80 ℃, and under nitrogen atmosphere or the dry air, dry 18-36 promptly obtained gallium nitrate in individual hour under the normal pressure.
Evidence, it can accomplish the end in view
Embodiment
Embodiment 1
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 9, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 15 hours repeatedly, till the solution that forms transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of water bath heating underpressure distillation 16 hours, removes most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 55 ℃, and system pressure is 0.05 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 50 ℃ of temperature, and under the nitrogen atmosphere, normal pressure both obtained gallium nitrate down in dry 36 hours.
Embodiment 2
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 15, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 12 hours repeatedly, till the solution of transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of water bath heating underpressure distillation 12 hours, removes most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 65 ℃, and system pressure is 0.1 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 65 ℃ of temperature, and under the nitrogen atmosphere, normal pressure both obtained gallium nitrate down in dry 30 hours.
Embodiment 3
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 18, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 8 hours repeatedly, till the solution that forms transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of heating in water bath underpressure distillation 10 hours, and removed most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 75 ℃, and system pressure is 0.2 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 75 ℃ of temperature, and under the nitrogen atmosphere, normal pressure both obtained gallium nitrate down in dry 20 hours.
Embodiment 4
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 9, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 15 hours repeatedly, till the solution that forms transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of water bath heating underpressure distillation 16 hours, removes most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 55 ℃, and system pressure is 0.05 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 55 ℃ of temperature, and under the dry air atmosphere, normal pressure both obtained gallium nitrate down in dry 34 hours.
Embodiment 5
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 9, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 15 hours repeatedly, till the solution that forms transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of water bath heating underpressure distillation 16 hours, removes most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 55 ℃, and system pressure is 0.05 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 60 ℃ of temperature, and under the dry air atmosphere, normal pressure both obtained gallium nitrate down in dry 32 hours.
Embodiment 6
A: Gallium trioxide is dissolved in salpeter solution, and the mol ratio of control Gallium trioxide and nitric acid is at 1: 9, during, add the water heating, continuous evaporating solns is after concentrating, add water again, this operation is 15 hours repeatedly, till the solution that forms transparent no obvious irritation smell.
B: the solution of a preparation was positioned under the condition of water bath heating underpressure distillation 16 hours, removes most of water and remaining nitric acid in the middle of the solution, obtain thick concentrated solution.During this time, control water temperature is at 55 ℃, and system pressure is 0.05 * 10
5Pa.
C: the thick concentrated solution that b is obtained is placed on 70 ℃ of temperature, and under the dry air atmosphere, normal pressure both obtained gallium nitrate down in dry 28 hours.
Present method is the feedstock production gallium nitrate with the gallium oxide of cheapness, and it is used to prepare the catalyzer of lean burn oxynitride control (as Ga
2O
3-Al
2O
3And SnO
2-Ga
2O
3-Al
2O
3Deng catalyst series), its performance can reach the level of import gallium nitrate fully, and cost is but less than one of percentage of import gallium nitrate cost.And this method preparation technology is simple, has good operability.
Claims (1)
1. the preparation method of gallium nitrate, this method contains the step of the inorganics of gallium being carried out nitric acid treatment, it is characterized in that, and it comprises following steps successively:
(1) Gallium trioxide is dissolved in salpeter solution, the mol ratio of control Gallium trioxide and nitric acid is 1: 6-18, during, adding water-heating-evaporation-concentrate-add water again, this operation is 6-15 hour repeatedly, until the transparent solution that has no irritating odor of formation;
(2) at water temperature 40-80 ℃, system pressure 0.05 * 10
5-0.5 * 10
5Under the Pa condition, the solution that step (1) is made was positioned under the condition of water bath heating underpressure distillation 8-16 hour, removed most of water and remaining nitric acid in the middle of the solution, obtained thick concentrated solution;
(3) the thick concentrated solution that step (2) is obtained is placed on temperature 40-80 ℃, and under nitrogen atmosphere or the dry air, dry 18-36 promptly obtained gallium nitrate in individual hour under the normal pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021241430A CN1178861C (en) | 2002-07-12 | 2002-07-12 | Method for preparing gallium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021241430A CN1178861C (en) | 2002-07-12 | 2002-07-12 | Method for preparing gallium nitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1467157A CN1467157A (en) | 2004-01-14 |
| CN1178861C true CN1178861C (en) | 2004-12-08 |
Family
ID=34142616
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021241430A Expired - Fee Related CN1178861C (en) | 2002-07-12 | 2002-07-12 | Method for preparing gallium nitrate |
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| Country | Link |
|---|---|
| CN (1) | CN1178861C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390068C (en) * | 2005-10-19 | 2008-05-28 | 中国石油化工股份有限公司 | Process for preparing gallium nitrate |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100398449C (en) * | 2006-03-16 | 2008-07-02 | 余泉茂 | Preparation method of gallium nitrate |
| JP2014019590A (en) * | 2012-07-13 | 2014-02-03 | Dowa Electronics Materials Co Ltd | Method for manufacturing aqueous gallium nitrate solution |
| CN102963923B (en) * | 2012-11-28 | 2015-04-15 | 南京金美镓业有限公司 | Large-scale production method for preparing gallium nitrate by using gallium |
| CN115650280A (en) * | 2022-09-09 | 2023-01-31 | 昆明理工大学 | Preparation method of gallium salt |
-
2002
- 2002-07-12 CN CNB021241430A patent/CN1178861C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390068C (en) * | 2005-10-19 | 2008-05-28 | 中国石油化工股份有限公司 | Process for preparing gallium nitrate |
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| Publication number | Publication date |
|---|---|
| CN1467157A (en) | 2004-01-14 |
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